US2450176A - Preparation of palladium oxide - Google Patents
Preparation of palladium oxide Download PDFInfo
- Publication number
- US2450176A US2450176A US769327A US76932747A US2450176A US 2450176 A US2450176 A US 2450176A US 769327 A US769327 A US 769327A US 76932747 A US76932747 A US 76932747A US 2450176 A US2450176 A US 2450176A
- Authority
- US
- United States
- Prior art keywords
- palladium
- palladium oxide
- silver
- oxide
- water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- 229910003445 palladium oxide Inorganic materials 0.000 title description 25
- 238000002360 preparation method Methods 0.000 title description 3
- JQPTYAILLJKUCY-UHFFFAOYSA-N palladium(ii) oxide Chemical compound [O-2].[Pd+2] JQPTYAILLJKUCY-UHFFFAOYSA-N 0.000 title 1
- HBEQXAKJSGXAIQ-UHFFFAOYSA-N oxopalladium Chemical compound [Pd]=O HBEQXAKJSGXAIQ-UHFFFAOYSA-N 0.000 description 24
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 18
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 14
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 13
- 229910052709 silver Inorganic materials 0.000 description 13
- 239000004332 silver Substances 0.000 description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- 229910052763 palladium Inorganic materials 0.000 description 10
- 229910001868 water Inorganic materials 0.000 description 10
- 229910001961 silver nitrate Inorganic materials 0.000 description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 7
- 229910017604 nitric acid Inorganic materials 0.000 description 7
- GPNDARIEYHPYAY-UHFFFAOYSA-N palladium(ii) nitrate Chemical compound [Pd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O GPNDARIEYHPYAY-UHFFFAOYSA-N 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 4
- 238000001704 evaporation Methods 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 238000009835 boiling Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 230000004927 fusion Effects 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- -1 palladium group metals Chemical class 0.000 description 3
- 239000000741 silica gel Substances 0.000 description 3
- 229910002027 silica gel Inorganic materials 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- 239000000956 alloy Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 150000002823 nitrates Chemical class 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000010970 precious metal Substances 0.000 description 2
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000007900 aqueous suspension Substances 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000010908 decantation Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000005350 fused silica glass Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000005297 pyrex Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/44—Palladium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/48—Silver or gold
- B01J23/50—Silver
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
Definitions
- This invention relates to the preparation of palladium oxide in a form useful as a catalyst.
- the method is particularly useful for obtaining thi compound from alloyed silver and palladium.
- Silver and palladium are extracted from gold and palladium group metals during refinement of the latter, by dissolving them from such precious metals with aqueous nitric acid. This produces an aqueous solution of silver and palladium nitrates, and the present invention may be used for preparing catalytic palladium oxide from such a solution. This i commercially advantageous in many instances.
- an aqueous solution of silver and palladium nitrates is evaporated to dryness.
- This solution may be obtained in connection with the refinement of precious metals as suggested above, or it may be produced only to practice the present invention as by dissolving silver and palladium in aqueous nitric acid.
- the corrosive nature of nitric acid should be kept in mind, it being suggested that the container in which the evaporation is carried out be.
- the dry residue obtained from the above evaporation step is heated to a temperature above the decomposition temperature of palladium nitrate and below the decomposition temperature of silver nitrate. Temperatures higher than 212 C. and lower than 440 C. are suitable for this purpose. At temperatures within this range the silver nitrate fuses and the palladium nitrate is decomposed to palladium oxide, it being understood that this heating step may be carried out with the crucible contents exposed to the atmosphere. As the temperatures described are maintained, the crucible contents will ultimately reach a state of quiescent fusion and the temperatures are maintained after this state is reached, for about minutes. Then the heating i discontinued and the melt cooled so it freezes.
- Example I aqueous solution containing about one gram of palladium and about nine grams of silver, both in the form of nitrates, was evaporated to dryness in a Pyrex (trade-mark) glass beaker. More heat was applied and the temperature gradually raised to about 220 C., and the heat was maintained at this temperature for about 10 minutes after an apparently quiet fusion was obtained. The fusion was cooled about or below the boiling temperature of water, and
- Example II About one gram of palladium and about nine grams of silver were melted together to form an alloy. This alloy was dissolved in about, 20 cc. of aqueous nitric acid, and then palladium oxide was prepared therefrom in exactly the same manner as in Example I.
- Example III -Supported Catalyst: Palladium oxide was prepared in exactly the same manner as described under Example I up to the point of filtering off the palladium oxide. Instead of filtering the palladium oxide, it was Washed with dilute aqueous nitric acid by decantation until substantially free from silver, and then it was washed with water. Thereafter about forty grams of silica gel was added to the aqueous suspension of palladium oxide left by retaining sufiicient water for this purpose. The mass of palladium oxide, water and silica gel was then heated to evaporate off the water. The mass was stirred during the heating process to obtain a uniform distribution of the palladium oxide on the surface of the silica gel.
- Example IV Supported Catalyst: Palladium oxide was prepared as in Example I except that about 10 grams of alumina were added to the mixed nitrates of silver and palladium before evaporation. In this manner the palladium oxide was deposited directly on the carrier as it was formed. Other carriers may be substituted for those employed in Examples III and IV.
- a method of preparing palladium oxide on a refractory support including mixing the support with an aqueous solution of palladium and silver nitrates, evaporating the water from the result and heating it to temperatures above the decomposition temperature of palladium nitrate and below the decomposition temperature of silver nitrate for a sufiicient time to decompose a. ubstantial portion of the palladium nitrate to Q alladium oxide and subjecting this result when cooled to the action of a. solvent of the silver niltrate but not of the palladium oxide to dissolve the former from the latter and to leave a deposit of the palladium oxide on said support.
- a method of preparing palladium oxide including the step of heating a mixture of palladium and silver nitrates to temperatures above that decomposing the palladium nitrate to pal-,
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
Description
Patented Sept. 28, 1948 v 2,450,176 PREPARATION OFPALLADIUM OXIDE .Herbert E. Zschiegner, Ocean Grove, N. J., as signor to EmanuelHonig, Brooklyn, N. Y.
No Drawing. Application August 18, 1947, Serial No; 769,327
2 Claims. (01. 252-472) This invention relates to the preparation of palladium oxide in a form useful as a catalyst. The method is particularly useful for obtaining thi compound from alloyed silver and palladium.
Silver and palladium are extracted from gold and palladium group metals during refinement of the latter, by dissolving them from such precious metals with aqueous nitric acid. This produces an aqueous solution of silver and palladium nitrates, and the present invention may be used for preparing catalytic palladium oxide from such a solution. This i commercially advantageous in many instances.
According to the invention, an aqueous solution of silver and palladium nitrates is evaporated to dryness. This solution may be obtained in connection with the refinement of precious metals as suggested above, or it may be produced only to practice the present invention as by dissolving silver and palladium in aqueous nitric acid. The corrosive nature of nitric acid should be kept in mind, it being suggested that the container in which the evaporation is carried out be.
made of platinum, tantalum, fused silica, stainless steel or one of the heat resistant glasses.
The dry residue obtained from the above evaporation step is heated to a temperature above the decomposition temperature of palladium nitrate and below the decomposition temperature of silver nitrate. Temperatures higher than 212 C. and lower than 440 C. are suitable for this purpose. At temperatures within this range the silver nitrate fuses and the palladium nitrate is decomposed to palladium oxide, it being understood that this heating step may be carried out with the crucible contents exposed to the atmosphere. As the temperatures described are maintained, the crucible contents will ultimately reach a state of quiescent fusion and the temperatures are maintained after this state is reached, for about minutes. Then the heating i discontinued and the melt cooled so it freezes.
After the temperature of the melt reduces to about or below water-boiling temperature, water is added to it and stirred until the silver nitrate is dissolved in the water, the palladium oxide being insoluble in water and forming a suspension in it. Thereafter the palladium oxide is mechanically separated, as by filtration, and is washed with aqueous nitric acid preferably in dilute solution, until free from silver. Then the palladium oxide is dried and is ready for use as Example I.-An aqueous solution containing about one gram of palladium and about nine grams of silver, both in the form of nitrates, was evaporated to dryness in a Pyrex (trade-mark) glass beaker. More heat was applied and the temperature gradually raised to about 220 C., and the heat was maintained at this temperature for about 10 minutes after an apparently quiet fusion was obtained. The fusion was cooled about or below the boiling temperature of water, and
about cc. of distilled water was added and heated to boiling. The resultant palladium oxide left as an insoluble mixture with the water, was filtered off after cooling enough for convenience, and Washed with dilute aqueous nitric acid until the filtrate was substantially free of silver.
Example II.About one gram of palladium and about nine grams of silver were melted together to form an alloy. This alloy was dissolved in about, 20 cc. of aqueous nitric acid, and then palladium oxide was prepared therefrom in exactly the same manner as in Example I.
Example III.-Supported Catalyst: Palladium oxide was prepared in exactly the same manner as described under Example I up to the point of filtering off the palladium oxide. Instead of filtering the palladium oxide, it was Washed with dilute aqueous nitric acid by decantation until substantially free from silver, and then it was washed with water. Thereafter about forty grams of silica gel was added to the aqueous suspension of palladium oxide left by retaining sufiicient water for this purpose. The mass of palladium oxide, water and silica gel was then heated to evaporate off the water. The mass was stirred during the heating process to obtain a uniform distribution of the palladium oxide on the surface of the silica gel.
Example IV.Supported Catalyst: Palladium oxide was prepared as in Example I except that about 10 grams of alumina were added to the mixed nitrates of silver and palladium before evaporation. In this manner the palladium oxide was deposited directly on the carrier as it was formed. Other carriers may be substituted for those employed in Examples III and IV.
The proportions given in the above examples are not critical and may be varied without departing from this invention. In all instances a satisfactory palladium oxide catalyst was produced. For ome purposes the silver need not be washed away completely.
I claim:
1. A method of preparing palladium oxide on a refractory support, including mixing the support with an aqueous solution of palladium and silver nitrates, evaporating the water from the result and heating it to temperatures above the decomposition temperature of palladium nitrate and below the decomposition temperature of silver nitrate for a sufiicient time to decompose a. ubstantial portion of the palladium nitrate to Q alladium oxide and subjecting this result when cooled to the action of a. solvent of the silver niltrate but not of the palladium oxide to dissolve the former from the latter and to leave a deposit of the palladium oxide on said support.
2. A method of preparing palladium oxide including the step of heating a mixture of palladium and silver nitrates to temperatures above that decomposing the palladium nitrate to pal-,
ladium oxide and below that decomposing the silver nitrate for a sufiicient time to decompose a substantial portion of the palladium nitrate, subjecting said mixture when cooled to the action of a solvent of the silver nitrate but not of the palladium oxide to dissolve the former from the latter and. to leave a suspension of the palladium oxide in the solvent, immersing a support in said suspension, and driving ofi the solvent to 5 deposit the palladium oxide on thesupport.
HERBERT E. ZSCHIE'GNER.
10 file of this patent:
UNITED STATES PATENTS Number Name Date Y 1,673,691 Lilfenroth June 18, 1928 '15 1,779,841 Fischer Oct. 28, 1930 2,043,743 Frary June 9, 1936
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US769327A US2450176A (en) | 1947-08-18 | 1947-08-18 | Preparation of palladium oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US769327A US2450176A (en) | 1947-08-18 | 1947-08-18 | Preparation of palladium oxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US2450176A true US2450176A (en) | 1948-09-28 |
Family
ID=25085121
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US769327A Expired - Lifetime US2450176A (en) | 1947-08-18 | 1947-08-18 | Preparation of palladium oxide |
Country Status (1)
| Country | Link |
|---|---|
| US (1) | US2450176A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2584756A (en) * | 1948-08-11 | 1952-02-05 | Socony Vacuum Oil Co Inc | Catalysis and process for reforming hydrocarbons |
| US3192168A (en) * | 1959-02-02 | 1965-06-29 | Rhone Poulenc Sa | Palladium-tin catalysts |
| US4501824A (en) * | 1982-02-01 | 1985-02-26 | Eltech Systems Corporation | Catalyst for making chlorine dioxide |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1673691A (en) * | 1923-09-18 | 1928-06-12 | Phosphorus Hydrogen Company | Method of producing hydrogen |
| US1779841A (en) * | 1926-07-13 | 1930-10-28 | Oscar A Fischer | Process of separating metallic compounds |
| US2043743A (en) * | 1934-09-08 | 1936-06-09 | Aluminum Co Of America | Alumina production |
-
1947
- 1947-08-18 US US769327A patent/US2450176A/en not_active Expired - Lifetime
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1673691A (en) * | 1923-09-18 | 1928-06-12 | Phosphorus Hydrogen Company | Method of producing hydrogen |
| US1779841A (en) * | 1926-07-13 | 1930-10-28 | Oscar A Fischer | Process of separating metallic compounds |
| US2043743A (en) * | 1934-09-08 | 1936-06-09 | Aluminum Co Of America | Alumina production |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2584756A (en) * | 1948-08-11 | 1952-02-05 | Socony Vacuum Oil Co Inc | Catalysis and process for reforming hydrocarbons |
| US3192168A (en) * | 1959-02-02 | 1965-06-29 | Rhone Poulenc Sa | Palladium-tin catalysts |
| US4501824A (en) * | 1982-02-01 | 1985-02-26 | Eltech Systems Corporation | Catalyst for making chlorine dioxide |
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